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Method for preparing 1, 4-butanediol through hydrogenation of 1, 4-butynediol

A technology of butynediol and butanediol, which is applied in the field of 1,4-butanediol production, can solve problems such as increasing system energy consumption, and achieve the effects of size reduction, investment reduction, and energy consumption reduction.

Pending Publication Date: 2022-04-29
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The above process has been disclosed many times in the prior art, but in the process of hydrogenation in the second stage, due to the heat removal requirements of the traditional fixed-bed trickle reaction system, the hydrogenation process with low concentration and large flow rate is still used. There is a large amount of water (60wt% ~ 70wt%) in the system, thus increasing the energy consumption of the system

Method used

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  • Method for preparing 1, 4-butanediol through hydrogenation of 1, 4-butynediol
  • Method for preparing 1, 4-butanediol through hydrogenation of 1, 4-butynediol

Examples

Experimental program
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Effect test

Embodiment 1

[0037] In this example, the composition of the Raney nickel-aluminum-X catalyst used in the low-pressure reactor R1: the mass ratio of nickel to aluminum is 0.5:1, and the amount of X added is 1wt% of the total mass of nickel and aluminum, wherein X is Mg . The preparation process is as follows: Weigh 250kg of Ni block, 500kg of Al block and 7.5kg of Mg and place them in a medium-to-large furnace, turn on the current, and after Ni, Al and Mg are melted, heat-preserve and smelt at 900°C for 60 minutes, then pour into Cool in water; grind the catalyst obtained after cooling to 200 mesh powder; weigh appropriate amount of catalyst powder in batches and add to NaOH solution with a mass concentration of 25% to mix evenly, then control the temperature at 60°C for 30 minutes, and react After finishing, wash 3 times with distilled water, then wash with absolute ethanol until neutral.

[0038] The composition of the catalyst loaded in the chilled water deheating tubular reactor R2 is ...

Embodiment 2

[0048] In this example, the composition of the Raney nickel-aluminum-X catalyst used in the low-pressure reactor R1: the mass ratio of nickel and aluminum is 0.6:1, and the amount of X added is 1wt% of the total mass of nickel and aluminum, wherein X is Mg . The preparation process is as follows: Weigh 300kg of Ni block, 500kg of Al block and 8kg of Mg and place them in a medium-to-large melting furnace, turn on the current, and after Ni, Al and Mg are melted, keep smelting at 900°C for 60 minutes, then pour into water Cooling; the catalyst obtained after cooling was ground to 200 mesh powder; weighed an appropriate amount of catalyst powder in batches and added to the NaOH solution with a mass concentration of 25% to mix evenly, then controlled the temperature at 60°C for 30 minutes, and the reaction was completed Afterwards, wash with distilled water 3 times, and then wash with absolute ethanol until neutral.

[0049] The composition of the catalyst loaded in the chilled wa...

Embodiment 3

[0055]In this example, the composition of the Raney nickel-aluminum-X catalyst used in the low-pressure reactor R1: the mass ratio of nickel and aluminum is 0.7:1, and the amount of X added is 1wt% of the total mass of nickel and aluminum, wherein X is Mg . The production process is as follows: Weigh 350kg of Ni block, 500kg of Al block and 8.5kg of Mg and place them in a medium-to-large furnace, turn on the current, and after Ni, Al and Mg are melted, heat-preserve and smelt at 900°C for 60 minutes, then pour into Cool in water; grind the catalyst obtained after cooling to 200 mesh powder; weigh appropriate amount of catalyst powder in batches and add to NaOH solution with a mass concentration of 25% to mix evenly, then control the temperature at 60°C for 30 minutes, and react After finishing, wash 3 times with distilled water, then wash with absolute ethanol until neutral;

[0056] The composition of the catalyst loaded in the chilled water deheating tubular reactor R2 is a...

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Abstract

The invention relates to a method for preparing 1, 4-butanediol by hydrogenation of 1, 4-butynediol, which comprises the following steps: a pressurized 1, 4-butynediol aqueous solution enters a low-pressure reactor, a hydrogenation reaction product in the first step is decompressed and then enters a normal-pressure cyclone separator, a reaction liquid is extracted from the top of the separator, and catalyst particles in the reaction liquid are further removed through a bag filter; the reaction liquid enters a pre-separation tower, the reaction liquid is segmented in a vacuum state, water, n-butyl alcohol and light components are distilled off from the tower top, and a mixed aqueous solution containing 1, 4-butanediol, 1, 4-butylene glycol, hydroxybutyraldehyde, acetal and heavy components is discharged from the tower bottom; the mixed aqueous solution enters a chilled water heat removal tubular reactor after being pressurized and preheated by a high-pressure hydrogenation preheater, the mixed aqueous solution is converted into 1, 4-butanediol under the action of a catalyst, reactants are extracted from the bottom of the reactor and then distilled to obtain a 1, 4-butanediol product, and the purpose of reducing energy consumption is achieved by separating in advance and changing the form of the hydrogenation reactor.

Description

technical field [0001] The invention relates to a production method of 1,4-butanediol, in particular to a method for preparing 1,4-butanediol by hydrogenating 1,4-butynediol. Background technique [0002] 1,4-Butanediol (abbreviated as BDO) is an important organic and fine chemical raw material, which is widely used in the fields of medicine, chemical industry, textile, papermaking, automobile and daily chemical industry. Tetrahydrofuran (THF), polybutylene terephthalate (PBT), gamma-butyrolactone (GBL) and polyurethane resin (PU Resin), coatings and plasticizers can be produced from 1,4-butanediol , and as a solvent and brightener in the electroplating industry, etc. [0003] Before World War II, Germany had adopted the Repp method to synthesize 1,4-butanediol from acetylene and formaldehyde. This method solves the danger of acetylene operating under high pressure, and it is still the most important production method of 1,4-butanediol. In the 1960s, Mitsubishi Petrochemi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/17C07C29/80C07C31/20B01J25/02B01J23/83B01J23/755
CPCC07C29/172C07C29/80B01J25/02B01J23/83B01J23/755B01J23/002B01J2523/00C07C31/207B01J2523/22B01J2523/31B01J2523/847B01J2523/3706B01J2523/17
Inventor 赵永祥刘绍波李海涛
Owner SHANXI UNIV
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