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Method for preparing 2-methyltetrahydrofuran catalyst through liquid phase hydrogenation of 2-methyl furan

A methyl tetrahydrofuran catalyst, methyl furan liquid technology, applied in the direction of heterogeneous catalyst chemical elements, catalyst supports, metal/metal oxide/metal hydroxide catalysts, etc., can solve harsh reaction conditions, contain precious metal production costs , high price and other problems, to achieve the effect of strong metal carrier interaction

Inactive Publication Date: 2019-08-30
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The diol method usually uses 2-methyl-1,4-butanediol as a raw material to obtain 2-methyltetrahydrofuran through intramolecular dehydration, but 2-methyl-1,4-butanediol is expensive and difficult to realize industrialization ; Lactone method is in SiHCl 3 In the presence of γ-rays or ultraviolet light to irradiate the lactone, 2-methyltetrahydrofuran is obtained. The reaction conditions of this method are harsh and it is easy to cause metal pollution; for the levulinic acid method, the catalyst used is usually a noble metal catalyst containing Pt or Pd , leading to higher production costs; and the furfural method has been extensively studied because of its easy-to-obtain raw materials, but the second-step hydrogenation reaction of the furfural method mainly uses precious metals as catalysts and is carried out under high pressure conditions, which is not conducive to reducing industrial Cost of production
Although the 2-methyltetrahydrofuran obtained by the above method maintains good activity, selectivity and stability, there are also some disadvantages such as the reaction being a liquid phase reaction that cannot be carried out continuously, the catalyst containing precious metals and the reaction under high pressure. The cost increases, these factors make it impossible to apply industrially

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0017] Example 1 weighs 33.0g of silica sol and 3.08g of zirconium oxychloride (ZrOCI 2 ·8H 2 O) The solids were dissolved in 120.5 g of water, respectively. Take 25.0g of glacial acetic acid drop by drop into the silica sol to generate Si(OH) 4 ; Get 20.0g of ammonia water drop by drop into ZrOCI 2 ·8H 2 In O solution, Zr(OH) is generated 4 precipitation. Mix the two precipitates, stir, and age at 80°C for 12 hours, then filter, wash, and roast the precipitates to obtain ZrO 2 -SiO 2 Carrier: Dissolve 15.8g of hydrated nickel nitrate in 130g of water, impregnate the carrier with hydrated nickel nitrate, immerse the carrier in excess impregnation solution, stir slowly and let it stand, dry at 120°C for 12h, and bake at 650°C for 4h. Get the finished catalyst.

example 2

[0018] Example 2 takes by weighing 44.0g of silica sol and 4.11g of zirconium oxychloride (ZrOCI 2 ·8H 2 O) The solids were dissolved in 135 g of water, respectively. Take 20.0g of glacial acetic acid drop by drop into the silica sol to generate Si(OH) 4 ; Get 28.0g ammonia water drop by drop into ZrOCI 2 ·8H 2 In O solution, Zr(OH) is generated 4 precipitation. Mix the two precipitates, stir, and age at 80°C for 12 hours, then filter, wash, and roast the precipitates to obtain ZrO 2 -SiO 2 Carrier: Dissolve 17.9g of hydrated nickel nitrate in 160g of water, impregnate the carrier with hydrated nickel nitrate, immerse the carrier in excess impregnation solution, stir slowly and let it stand, dry at 120°C for 12h, and bake at 600°C for 4h. Get the finished catalyst.

example 3

[0019] Example 3 takes by weighing 59.0g of silica sol and 5.14g of zirconium oxychloride (ZrOCI 2 ·8H 2 O) The solids were dissolved in 130 g of water, respectively. Take 15.0g of glacial acetic acid drop by drop into the silica sol to generate Si(OH) 4 ; Get 23.0g ammonia water drop by drop into ZrOCI 2 ·8H 2 In O solution, Zr(OH) is generated 4 precipitation. Mix the two precipitates, stir, and age at 80°C for 12 hours, then filter, wash, and roast the precipitates to obtain ZrO 2 -SiO 2 Carrier: Dissolve 16.7g of hydrated nickel nitrate in 145g of water, impregnate the carrier with hydrated nickel nitrate, immerse the carrier in excess impregnation solution, stir slowly and let it stand, dry at 120°C for 12h, and roast at 675°C for 4h. Get the finished catalyst.

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PUM

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Abstract

The invention provides a method for preparing a 2-methyltetrahydrofuran catalyst through liquid phase hydrogenation of 2-methyl furan, and relates to a catalyst preparation method, which comprises: weighing a silica sol; taking glacial acetic acid, and adding into the silica sol in a dropwise manner; taking zirconium oxychloride (ZrOCI2.8H2O), and dissolving in deionized water; taking ammonia water, and adding into the ZrOCI2.8H2O solution in a dropwise manner; mixing the two precipitates, stirring, and aging for 12 h at a temperature of 80 DEG C; filtering the precipitate, washing, and calcining to obtain a ZrO2-SiO2 carrier; and preparing a catalyst, wherein the ZrO2-SiO2 solid powder is accurately weighed as the carrier, a soluble nickel salt and the soluble salts of other metals are taken and dissolved in water as an impregnation liquid, the carrier is immersed in the excess impregnation liquid, slow stirring and complete standing are sequentially performed, the excess solution isdrained after the adsorption equilibrium is achieved, the obtained material is dried, and the dried material is calcined to completely activate so as to prepare the finished NiO / ZrO2-SiO2 catalyst, wherein the mass percentage of NiO is 30%, and the mass percentage of the metal aid is 0.2-8%. According to the present invention, the used active component is non-precious metal Ni, and the carrier isZrO2-SiO2, such that the activity, the selectivity and the stability of the catalyst are substantially improved.

Description

technical field [0001] The invention relates to a method for preparing a catalyst, in particular to a method for preparing a 2-methyltetrahydrofuran catalyst by liquid-phase hydrogenation of 2-methylfuran. Background technique [0002] 2-Methyltetrahydrofuran is an important biogasoline fuel, chemical intermediate and high-end environmentally friendly solvent. As a bio-gasoline fuel, 2-methyltetrahydrofuran can replace part of gasoline as an automotive fuel additive, can be miscible with gasoline in any proportion, and has excellent oxidation and vapor pressure properties. Studies have shown that its proportion in gasoline can exceed 60% by volume, and it will not have any impact on engine performance, and the fuel consumption of automobiles will not increase. Using it as a gasoline additive can have higher economic value. In addition, 2-methyltetrahydrofuran can also be used as a co-solvent for ethanol, which can reduce the pressure of ethanol and increase the mixing ratio...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J21/08C07D307/06B01J32/00
CPCB01J21/08B01J23/002B01J23/755B01J2523/00C07D307/06B01J2523/41B01J2523/48B01J2523/847
Inventor 张雅静王子王罗澜乔宜扬
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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