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Selective hydrogenation catalyst and preparation method and application thereof

A hydrogenation catalyst and catalyst technology, applied in hydrogenation preparation, chemical instruments and methods, metal/metal oxide/metal hydroxide catalyst, etc., can solve problems such as increasing the amount of active components and reducing catalyst activity

Inactive Publication Date: 2010-08-25
中国中化股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this way, there is an unavoidable problem in the existing catalysts: on the one hand, in order to increase the reaction activity and the conversion rate of acetylenes, the amount of active components is increased; Activity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0013] Catalyst preparation: 105 g PdCl 2 (Pd content 59.5%), add 150 milliliters of 37% hydrochloric acid, 1600 milliliters of water, after heating and dissolving, adjust pH=4-5 with 30% sodium hydroxide solution for later use. In a 50-liter reactor, add 6300 grams of calcium carbonate and 22 liters of water, stir and heat until the temperature reaches 70°C, then add the pre-prepared palladium chloride solution dropwise. Finish dripping in 3 hours and keep for 30 minutes. Then add 600 ml of 0.7 mol / L sodium formate solution, and react at 75° C. for 1 hour. Cool down and filter, the filter cake is washed six times, each 1000 ml, and discharged. The wet product was put into an enamel tray and baked in an oven at 140° C. for 10 hours to obtain a finished catalyst with a palladium content of 1%.

example 2

[0017] Catalyst preparation: 100 g PdCl 2 (Pd content 59.5%), add 150 milliliters of 37% hydrochloric acid, 2000 milliliters of water, after heating and dissolving, adjust pH=4-5 with 30% sodium hydroxide solution for later use. In a 50-liter reactor, add 6,500 grams of barium sulfate and 25 liters of water, stir and heat to 70°C, then add the pre-prepared palladium chloride solution dropwise. Finish dripping in 3 hours and keep for 30 minutes. Then add 630 ml of 0.7 mol / L sodium formate solution, and react at 75° C. for 1 hour. Cool down and filter, the filter cake is washed six times, each 1000 ml, and discharged. The wet product was placed in an enamel tray in an oven at 140°C for 8 hours. The palladium content of the catalyst was 0.91%.

[0018] Application example: Add 2.5 kg of the above catalyst, 750 kg of 1,4-butynediol and 250 kg of water into a 2000-liter autoclave. The autoclave was replaced with nitrogen and hydrogen 4 times successively. Continuously feed hy...

example 3

[0021] The preparation of the catalyst was the same as in Example 1, and the palladium content was adjusted to be 0.8%.

[0022] Application example: Add 3 kg of the above catalyst, 700 kg of 1,4-butynediol and 300 kg of water into a 2000-liter autoclave. The autoclave was replaced with nitrogen and hydrogen 4 times successively. Continuously feed hydrogen and keep the hydrogen pressure at 0.4Mpa, and control the reaction temperature at 95-105°C until no hydrogen is absorbed as the end point of the reaction. The temperature is lowered, and the catalyst is separated by filtration and returned to the autoclave for recycling. Filtrate obtains 704 kilograms of products through vacuum dehydration, and through analysis (analysis method is the same as above), wherein 1,4-butenediol content is 98.2% (wherein cis content is 96.3%, trans content is 1.9%), 1,4- Butynediol content is 0.12%, 1,4-butanediol content is 0.35%.

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PUM

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Abstract

The invention discloses a selective hydrogenation catalyst and a preparation method and application thereof. The catalyst comprises the following components: palladium is used as an active ingredient without the addition of a second component; calcium carbonate or barium sulfate is used as a carrier; and the palladium content of the catalyst is 0.5 to 1.5 weight percent. The selective hydrogenation catalyst prepared according to the provided method has high activity and good selectivity. When the catalyst is applied to 1,4-butynediol reduction reaction, the conversion rate of 1,4-butynediol can reach over 99.8 percent; and the selectivity of the 1,4-butynediol is over 98 percent.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and relates to a selective hydrogenation catalyst and its preparation method and application. Specifically, it relates to a palladium active component selective hydrogenation catalyst, a preparation method of the catalyst, and an application of the catalyst to 1,4-butynediol catalytic hydrogenation to prepare 1,4-butenediol. technical background [0002] 1,4-butenediol is widely used in the synthesis of drugs vitamin VB 6 Intermediates can also be used in the synthesis of 1,2,4-butanetriol. Since the 1970s, Lindella catalysts have been used to prepare 1,4-butenediol. [0003] Lindra catalyst (Pd-Pb / CaCO 3 ) has been widely used in organic synthesis and chemical production since its composition and preparation method were disclosed (Org.Synth.1966, 48:89-92). The poisoning effect of the Pb component and the additive quinoline played a key role in inhibiting the further reduction of the formed ...

Claims

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Application Information

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IPC IPC(8): B01J23/44C07C33/035C07C29/17
Inventor 李付刚李文骁张丽莉
Owner 中国中化股份有限公司
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