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Green synthesis of 2-methylte-trahydrofuran

A methyltetrahydrofuran, green synthesis technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, organic chemistry and other directions, can solve problems such as high reaction pressure catalysts, and achieve good popularization and application Prospect, less usage, better response to stress

Active Publication Date: 2009-07-29
ZHEJIANG UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The purpose of the present invention is to provide a green synthesis method for preparing 2-methyltetrahydrofuran by using a high-efficiency and low-toxicity composite catalyst through liquid-phase catalytic hydrogenation of 2-methylfuran under lower reaction pressure, so as to solve the problem of prior art reaction Problems with excessive pressure or use of catalysts with toxic components

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0030] Preparation of ruthenium and a non-noble metal zinc simultaneously loaded on the catalyst of activated carbon carrier: 3%Ru.5%Zn / C. The operation steps are as follows: Weigh 0.62g of RuCl 3 and 1.05g ZnCl 2 , add pure water to make a 300mL aqueous solution, pour it into a 500mL 3-necked flask, then add 10.0g of activated carbon carrier, seal it and let it stand in a constant temperature water bath at 25°C for 12 hours, then raise the temperature to 50°C and stir for 2 hours. Then use NaOH to adjust the pH value of the solution to 9, then use analytically pure formaldehyde to reduce and filter, and wash the filter cake with deionized water until there is no chloride ion in the filtrate. After suction filtration, put the filter cake in a vacuum oven and dry it at 100°C for 3 hours That is the composite catalyst.

[0031] Preparation of 2-MeTHF: In a pressure reactor, add 100g of MeF and 1g (1% of the mass of MeF) of the composite catalyst prepared above, and carry out a ...

Embodiment 2-4

[0033] Change the mass ratio of the catalyst 3%Ru.5%Zn / C to 2-methylfuran in Example 1, as well as the reaction temperature and reaction pressure. Other operations are as in Example 1. The experimental conditions and experimental results are shown in Table 1.

[0034] Table 1 The reaction results of 3%Ru.5%Zn / C composite catalyst

[0035]

[0036]

Embodiment 5-9

[0038] Preparation of 12% Ru.10% Zn / C composite catalyst: RuCl 3 and ZnCl 2 Change the consumption of 2.48g and 2.10g into, and all the other operation steps are with embodiment 1. Use this composite catalyst to carry out hydrogenation reaction, change the mass ratio of catalyst and 2-methylfuran, reaction temperature and reaction pressure, other operations are as in Example 1, and the experimental conditions and experimental results are shown in Table 2.

[0039] Table 2 Reaction results of 12%Ru.10%Zn / C composite catalyst

[0040]

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Abstract

The invention discloses a green synthetic method of 2-methyltetrahydrofuran as is shown in formula (I): in a pressure reaction kettle, the liquid phase hydrogenation is carried out on the 2-methyltetrahydrofuran shown in formula (II) and composite catalysts at the reaction temperature of 50-100 DEG C and the reaction pressure of 1.0-4.0MPa until hydrogen is absorbed completely, and after the reaction is finished, reaction liquid is separated to obtain the 2-methyltetrahydrofuran as is shown in the formula (I); the composite catalysts are noble metal and non-noble metal simultaneously loaded on an activated carbon support. The noble metal is ruthenium, and the non-noble metal is one or more than one of zinc, copper or iron. As a green chemical synthetic method with perfect extension and application prospect, the green synthetic method of the 2-methyltetrahydrofuran provided by the invention has the advantages of little noble metal usage in the catalysts, low catalyst preparing cost, low reaction pressure, proper temperature, convenient operation, high yield, pollution-free property, easy recovery of the catalysts, etc.

Description

(1) Technical field [0001] The invention relates to a green synthesis method of 2-methyltetrahydrofuran. (2) Background technology [0002] 2-Methyltetrahydrofuran (hereinafter referred to as 2-MeTHF) is an important organic synthesis intermediate and solvent, and belongs to fine chemical materials in the field of new materials and applications. In organic synthesis, it is mainly used in the synthesis of chloroquine phosphate, primaquine phosphate and thiamine. In terms of solvent application, it is mainly used for organic synthesis of resin, natural rubber, ethyl cellulose and chloroacetic acid-vinyl acetate copolymer. As a cyclic ether, 2-MeTHF is also a Lewis base, and it is a unique solvent with environmental friendliness and excellent performance. In recent years, due to the excellent performance and environment-friendly characteristics of 2-MeTHF, it has developed rapidly in the field of solvent replacement applications: ① It is used to replace tetrahydrofuran and et...

Claims

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Application Information

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IPC IPC(8): C07D307/06B01J23/60B01J23/89
CPCY02P20/584
Inventor 苏为科李振华邵建华应素华王凌云王天发
Owner ZHEJIANG UNIV OF TECH
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