Preparation method and activation method of Raney nickel-aluminum-X catalyst specially for hydrogenation preparation of 1,4-butanediol from 1,4-butynediol

A technology of butynediol and activation method, which is applied in the field of preparation and activation of Raney nickel-aluminum-X catalysts, can solve the problems affecting the purity of catalyst active products, and achieve easy crushing, simple preparation method and high catalytic effect Effect

Active Publication Date: 2012-10-24
HAISO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the disadvantage of easily introducing other harmful ions, affecting the activity of the catalyst and the purity of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 250g of Ni block, 500g of Al block and 0.75g of B respectively and place them in an intermediate frequency induction furnace, turn on the current, after Ni, Al and X are melted, after melting at 900°C for 60 minutes, pour into water to cool; The catalyst obtained after grinding to 200 mesh powder; Weigh 200g of catalyst powder and add in batches 400g of NaOH solution with a mass concentration of 25% and mix evenly, then control the temperature at 60°C for 30min, after the reaction is completed, wash with distilled water 3 times, and then washed with absolute ethanol until neutral; the whole activation process was controlled for 2h; the activated catalyst was moved into a high-pressure reactor with 3000g 35wt% 1,4-butynediol solution inside, and the reaction pressure was 3MPa , the reaction temperature was 50°C, and the stirring speed was 1500 rpm for 3 hours. The conversion rate of 1,4-butynediol was 98.3%, and the selectivity of 1,4-butanediol was 90.8%.

Embodiment 2

[0026] Weigh 250g of Ni block, 500g of Al block and 0.75g of Mg and place them in the medium frequency induction furnace, turn on the current, after Ni, Al and X are melted, after melting at 900°C for 60min, pour into water to cool; The catalyst obtained after grinding to 200 mesh powder; Weigh 200g of catalyst powder and add in batches 400g of NaOH solution with a mass concentration of 25% and mix evenly, then control the temperature at 60°C for 30min, after the reaction is completed, wash with distilled water 3 times, and then washed with absolute ethanol until neutral; the whole activation process was controlled for 2h; the activated catalyst was moved into a high-pressure reactor with 3000g 35wt% 1,4-butynediol solution inside, and the reaction pressure was 3MPa , the reaction temperature was 50°C, and the stirring speed was 1500 rpm for 3 hours. The conversion rate of 1,4-butynediol was 98.7%, and the selectivity of 1,4-butanediol was 92.8%.

Embodiment 3

[0028] Weigh 300g of Ni block, 500g of Al block and 1.6g of Sr respectively and put them in the medium frequency induction furnace, turn on the current, after Ni, Al and X are melted, after smelting at 1000℃ for 60min, pour into water to cool; The obtained catalyst was ground to 200-mesh powder; weighed 200g of catalyst powder and added in batches to 400g of KOH solution with a mass concentration of 25% and mixed evenly, then controlled the temperature at 60°C for 30min, after the reaction was completed, washed with distilled water 3 times, and then washed with absolute ethanol until neutral; the whole activation process was controlled for 2h; the activated catalyst was moved into a high-pressure reactor with 3000g 35wt% 1,4-butynediol solution inside, and the reaction pressure was 3MPa , the reaction temperature was 50°C, and the stirring speed was 1500 rpm for 3 hours. The conversion rate of 1,4-butynediol was 98.7%, and the selectivity of 1,4-butanediol was 93.5%.

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Abstract

The invention discloses a preparation method and an activation method of a Raney nickel-aluminum-X catalyst specially for hydrogenation preparation of 1,4-butanediol from 1,4-butynediol. The Raney nickel-aluminum-X catalyst is characterized in that a mass ratio of nickel to aluminum is (0.5 to 1): 1; X of which mass is 0.1 to 2% of total mass of nickel and aluminum is adopted; and X represents Mg, B, Sr, Cr, S, Ti, La, Sn, W, Mo or Fe. The preparation method comprises the following steps of putting nickel, aluminum and X into a medium frequency induction smelting furnace according to the mass ratio, carrying out smelting, pouring out melt, cooling, crushing, and grinding to obtain powder which is the Raney nickel-aluminum-X catalyst. The activation method comprises the following steps that an alkali solution and the Raney nickel-aluminum-X catalyst which is powder are uniformly mixed according to a mass ratio of (2: 1) to (10: 1) and then undergo a reaction with stirring, wherein the alkali solution is a sodium hydroxide or potassium hydroxide solution having a concentration of 5 to 25wt%; after the reaction is finished, the reaction products are washed by distilled water and anhydrous ethanol until a pH value of the reaction products is 7; and the reaction products having a pH value of 7 are preserved in ethanol. In the presence of the Raney nickel-aluminum-X catalyst, in hydrogenation preparation of 1,4-butanediol from 1,4-butynediol, a conversion rate is in a range of 98 to 100% and selectivity of 1,4-butanediol is in a range of 90 to 98%.

Description

technical field [0001] The invention belongs to the field of organic chemical catalysts, in particular to a preparation and activation method of a Raney nickel-aluminum-X catalyst specially used for hydrogenating 1,4-butynediol to 1,4-butanediol. Background technique [0002] 1,4-Butanediol (BDO) is a very important intermediate in organic synthesis, widely used in the production of polytetramethylene glycol ether (PTMEG), polybutylene terephthalate (PBT) , Tetrahydrofuran (THF) and other fields as well as the pharmaceutical and cosmetic industries. At present, there are many processes for producing BDO in the world, among which the Reppe method is the most widely used, that is, firstly, 1,4-butynediol is prepared from formaldehyde and acetylene, and then 1,4-butynediol is hydrogenated to form butanediol. Alcohol method. In the process for preparing butanediol by hydrogenation of butynediol disclosed in U.S. Patent 2967893, the catalyst used is to add a certain proportio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J25/02B01J37/00B01J25/04C07C29/17C07C31/20
CPCY02P20/584
Inventor 胡燕李耀会章小林张雄斌李新怀吕小婉李小定
Owner HAISO TECH
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