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Hydrogenation catalyst, preparation method of hydrogenation catalyst and application of hydrogenation catalyst to 2-methyltetrahydrofuran synthesis

A technology for hydrogenation catalysts and compounds, applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of unsatisfactory 2-methyltetrahydrofuran yield, The difficulty of in-situ regeneration of the copper catalyst is increased, and the production is difficult to proceed smoothly, so as to achieve the effects of reducing energy consumption, simple preparation method, and improving selectivity

Active Publication Date: 2013-02-13
JIANGSU QINGQUAN CHEM CO LTD
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, in this method, the decline in the activity of any catalyst will lead to a reduction in the efficiency of the entire device, making it difficult to carry out production smoothly; at the same time, the in-situ regeneration of the copper catalyst is more difficult, and the precious metal palladium catalyst is exposed to materials containing a large amount of impurities for a long time. Inactivate
[0009] Adopt the method of above-mentioned one-step hydrogenation of furfural, can reduce the rectification step of high energy consumption, but the yield of preparing 2-methyltetrahydrofuran is still not ideal

Method used

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  • Hydrogenation catalyst, preparation method of hydrogenation catalyst and application of hydrogenation catalyst to 2-methyltetrahydrofuran synthesis
  • Hydrogenation catalyst, preparation method of hydrogenation catalyst and application of hydrogenation catalyst to 2-methyltetrahydrofuran synthesis

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preparation example Construction

[0024] According to the present invention, the preparation method of the hydrogenation catalyst comprises: combining a soluble compound of hydrogenation active component ruthenium, Mn or Mn with at least one metal component selected from Group IB, Group IIB, Group IIIB and Group VIII The combination of soluble compounds with ZrO as auxiliary2 The composite carrier of ZnO is uniformly mixed in water to obtain a mixture, and the mixture is contacted with a reducing agent capable of reducing ruthenium ions in the soluble compound of ruthenium and metal ions in the soluble compound of the auxiliary agent, and filtered to obtain a solid precipitate . The method of uniformly mixing the soluble compound of ruthenium and the soluble compound of the auxiliary agent with the carrier in water can be carried out in the following two ways: (1) the soluble compound of ruthenium and the soluble compound of the auxiliary agent can be mixed with the carrier, and then uniformly mixed in water M...

Embodiment 1

[0057] (1) Carrier preparation

[0058] At 40°C, 100g of zirconium oxychloride octahydrate and 132g of zinc nitrate hexahydrate were dissolved in 500mL of water, stirred to dissolve completely, and 1400g of 12% by weight sodium carbonate solution was added dropwise to the solution to adjust the pH to 9.6; Raise the temperature to 95°C and age for 2h. Filter and wash with deionized water until no chloride ions are detected by silver nitrate; the filter cake is dried at 100°C and calcined at 600°C for 3.5h to obtain 70g of solid.

[0059] (2) Catalyst preparation

[0060] Mix 1.5 g of an aqueous ruthenium chloride solution with a metal ruthenium concentration of 10% by weight, 1.6 g of a 50% by weight manganese nitrate aqueous solution, and 50 mL of distilled water, and stir for 30 min. Then add 5 g of the carrier prepared in the above step (1), and stir for 1 h. Under stirring condition, add dropwise 33mL of 0.5mol / LKBH 4 The aqueous solution was added dropwise within 10-15...

Embodiment 2

[0062] (1) Carrier preparation

[0063] At 30°C, 200g of zirconium oxychloride octahydrate and 132g of zinc nitrate hexahydrate were dissolved in 500mL of water, and stirred to completely dissolve it; 2000g of 12% by weight sodium carbonate solution was added dropwise to the solution, and the terminal pH was 9.4; Raise the temperature to 90°C and age for 2.5 hours. Filter and wash with deionized water until no chloride ions are detected by silver nitrate; the filter cake is dried at 110°C and calcined at 550°C for 4.5h to obtain 107g of solid.

[0064] (2) Catalyst preparation

[0065] Prepare according to the catalyst preparation method of Example 1, the difference is that the carrier prepared in Example 2 is used. The hydrogenation catalyst C2 was obtained, the composition of which is shown in Table 1.

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Abstract

The invention discloses a hydrogenation catalyst which contains a carrier, an active component and an auxiliary. The active component and the auxiliary are loaded on the carrier, wherein the active component is ruthenium (Ru), the auxiliary is manganese (Mn) or a combination of Mn and at least one of metal components of an IB group, an IIB group, an IIIB group and a VIII group, and the carrier is a composite carrier of ZrO2 and ZnO. The invention further provides a preparation method of the hydrogenation catalyst and an application of the hydrogenation catalyst to 2-methyltetrahydrofuran synthesis. The hydrogenation catalyst has higher catalytic activity and 2-methyltetrahydrofuran selectivity and longer service life in the reaction that raw materials containing 2-methyl furan synthesize the 2-methyltetrahydrofuran through hydrogenation, and the raw materials containing the 2-methyl furan are not required to be rectified so that process is simplified, and energy consumption is reduced.

Description

technical field [0001] The invention relates to a hydrogenation catalyst, a preparation method thereof and an application in synthesizing 2-methyltetrahydrofuran. Background technique [0002] 2-Methyltetrahydrofuran (2-MeTHF) is an important organic intermediate and an excellent solvent. Its boiling point is 80.2°C and its solubility in water is small, so it is easy to separate from water. At the same time, 2-Methyltetrahydrofuran It has a Lewis basicity similar to that of tetrahydrofuran, so it can be applied to many organometallic reactions. In addition, because 2-methyltetrahydrofuran can be miscible with gasoline in any ratio, it can also be used as an automobile fuel additive to replace part of gasoline. [0003] At present, 2-methyltetrahydrofuran is mainly synthesized by hydrogenation of furfural or furfuryl alcohol to 2-methylfuran, and then further prepared by hydrogenation of 2-methylfuran. However, industrially produced 2-methylfuran usually contains some impur...

Claims

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Application Information

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IPC IPC(8): B01J23/656B01J23/89C07D307/06
Inventor 朱兆火聂振中游梦云冯珍会符建琼张浩张潮潘智伟王立志
Owner JIANGSU QINGQUAN CHEM CO LTD
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