Ruthenium catalyst, preparation method and application in synthesizing tetrahydrofurfuryl alcohol

A technology of ruthenium catalyst and tetrahydrofurfuryl alcohol, applied in the field of ruthenium catalyst, its preparation and its application in the synthesis of tetrahydrofurfuryl alcohol, can solve the problems of high hydrogenation pressure, low hydrogenation activity, side reactions, etc., and achieve high conversion efficiency, high selectivity

Active Publication Date: 2012-06-13
JIANGSU QINGQUAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the reaction process, if the reaction temperature is low, the hydrogenation activity is low, and a very high hydrogenation pressure is required; and when the reaction temperature is raised, fur

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0015] Example 1

[0016] Catalyst preparation: 1.5g FeCl 3 .6H 2 O, 0.75g RuCl with 10% ruthenium metal concentration 3 The aqueous solution and 50ml of distilled water were added to a three-necked flask and fully dissolved under mechanical stirring for 30 minutes. Then add 0.5 g of non-ionic surfactant nonylphenol polyoxyethylene ether, stir for 5 minutes, add 2.1 g of titanium dioxide carrier, and stir for 1 hour. Weigh 0.8g KBH 4 Make 30ml water solution. Under stirring conditions, start adding KBH dropwise 4 The aqueous solution is controlled to be added dropwise within 10-15min and continue stirring for 0.5h. The above solution was centrifuged, and the precipitate was washed with distilled water until neutral. The above precipitate was activated in 100 ml of a 10% sodium sulfate aqueous solution at 120° C. and 1 MPa hydrogen pressure for 3 hours. After centrifugal separation and washing with ethanol 3 times, the target catalyst in this example was obtained.

[0017] One-s...

Example Embodiment

[0022] Example 2

[0023] The preparation of the catalyst is basically the same as in Example 1, but no surfactant is used. That is, compared with Example 1, the step of "adding 0.5 g of nonylphenol polyoxyethylene ether of non-ionic surfactant" is lacking. The process of one-step hydrogenation of furfural to synthesize tetrahydrofurfuryl alcohol is the same as in Example 1. The results of the reaction are shown in Table 1.

Example Embodiment

[0024] Example 3

[0025] The preparation of the catalyst is basically the same as in Example 1, but without using any metal promoters, while adding 10% RuCl 3 The amount of the aqueous solution was changed to 0.30g. In other words, the "1.5g FeCl 3 .6H 2 O, 0.75g RuCl with 10% ruthenium metal concentration 3 "Aqueous solution" is changed to "0.30g RuCl with 10% ruthenium metal concentration 3 Aqueous solution". The process of one-step hydrogenation of furfural to synthesize tetrahydrofurfuryl alcohol is the same as in Example 1. The reaction results are shown in Table 1.

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Abstract

The invention provides a ruthenium catalyst for synthesizing tetrahydrofurfuryl alcohol in one-step hydrogenation of furfural. The expression of the ruthenium catalyst is Ru-M/TiO2, wherein Ru accounts for 0.5-15 wt% of the catalyst; and M is a metal auxiliary and accounts for 0-20 wt% of the catalyst. A preparation method of the ruthenium catalyst comprises the following steps of: adding a carrier TiO2 into a water solution containing ruthenium salt or a water solution containing ruthenium salt and metal auxiliary salt such that the weight ratio of ruthenium to carrier is 0.005-0.15:1; and then, adding 2-10 wt% of potassium borohydride or hydrazine hydrate solution to precipitate the solution. A nonionic surfactant is optimally added in the preparation method to improve the catalytic activity and selectivity. If the catalyst is subject to hydro-thermal treatment in a water solution of sodium sulfate, then the adsorption property of the catalyst can be changed, and the selectivity of catalyzing furfural to synthesize tetrahydrofurfuryl alcohol through one-step hydrogenation can be greatly improved. The catalyst has simple preparation method, good catalytic activity and high selectivity and is especially applicable to catalyzing the reaction of furfural to synthesize tetrahydrofurfuryl alcohol through one-step hydrogenation under the conditions of low temperature, low pressure and no solvent. Under certain reaction conditions, the yield of tetrahydrofurfuryl alcohol can reach more than 99%.

Description

technical field [0001] The invention relates to a ruthenium catalyst, its preparation method and its application in synthesizing tetrahydrofurfuryl alcohol. Background technique [0002] Tetrahydrofurfuryl alcohol is an important chemical raw material with a wide range of uses. It can be used to prepare lysine, tetrahydrofuran, pyran and pyridine, etc. It can also be used to prepare herbicides, insecticides, antifreeze agents, plasticizers and decolorization. chemicals, etc. At present, tetrahydrofurfuryl alcohol in industry is mainly obtained by two-step hydrogenation of furfural. Wherein the first step is the hydrogenation of furfural to furfuryl alcohol, mainly using a copper-based catalyst, such as the traditional copper-chromium system disclosed in documents US2094975, CN1562477 and CN1978051 and the chromium-free systems such as copper-zinc-aluminum and copper-magnesium disclosed in documents CN1410161 and CN1256965; The yield of furfuryl alcohol can reach more than ...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J23/46B01J23/745B01J23/60B01J23/656C07D307/12
Inventor 宁剑波张锦红泮伟平陈欣荣朱骥徐卫军汤廷翔方彦中刘峰
Owner JIANGSU QINGQUAN CHEM CO LTD
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