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Combined alkaline iron-molybdenum sulfide catalyst, preparation method of catalyst and application of catalyst to aromatic phenol and ether conversion

A catalyst and composite technology, applied in the preparation of organic compounds, physical/chemical process catalysts, chemical instruments and methods, etc., to achieve the effect of improving activity

Active Publication Date: 2017-09-15
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, on the other hand, traditional sulfides must also have their advantages, and how to combine the two is a certain challenge

Method used

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  • Combined alkaline iron-molybdenum sulfide catalyst, preparation method of catalyst and application of catalyst to aromatic phenol and ether conversion
  • Combined alkaline iron-molybdenum sulfide catalyst, preparation method of catalyst and application of catalyst to aromatic phenol and ether conversion
  • Combined alkaline iron-molybdenum sulfide catalyst, preparation method of catalyst and application of catalyst to aromatic phenol and ether conversion

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] This example illustrates the preparation of hydrotalcites with different ratios in the present invention, taking Mg:Fe=3:1 as an example

[0029] (a) Weigh 21.77g (0.09mol) of magnesium nitrate, dissolve 12.12g (0.03mol) of ferric nitrate in 250ml of deionized water, stir until clear; weigh 9.6g (0.24mol) of sodium hydroxide, 6.36g (0.06mol) ) Sodium carbonate is dissolved in 250mol deionized water, stirred until clarification;

[0030] (b) Drop the two solutions into 500ml deionized water at the same time, stir in a 70°C water bath, and control the titration speed to ensure that the pH is between 9-10; after the titration, continue to stir for 120 minutes, and then transfer to the oven, The crystallization temperature was set at 70° C., and the crystallization time was 12 hours.

[0031] (c) After crystallization, filter and wash the precipitate with deionized water until the pH is neutral, and dry the obtained precipitate at 70°C for 12 hours to obtain Mg with an ato...

Embodiment 2

[0035] This example illustrates the preparation of hydrotalcite-based composite oxides in the present invention

[0036] The different proportions of hydrotalcites prepared in Example 1 were placed in a muffle furnace, the temperature rise program was set to 5-20K / min, and it was raised to 400°C to obtain the different proportions of Mg at this temperature x Fe y oxide.

[0037] Change the roasting temperature between 350-500°C to ensure that CO 3 2‐ removal while maintaining the recoverability of its structure.

Embodiment 3

[0039] The present embodiment illustrates the preparation of composite sulfide catalyst in the present invention

[0040] (a) Weigh 2.0g of ammonium heptamolybdate and dissolve it in 16mol deionized water, stir to form a clear solution, then weigh 1.0g of Mg obtained by calcining at 400°C in Example 3x Fe y Add the oxide to the solution, seal the mouth of the beaker with parafilm, ion exchange at room temperature for 12 hours, wash and dry to obtain MgxFey-MoO 4 2- precursor; then in 10% H 2 S / H 2 Sulphurization in a mixed gas, the sulphurization temperature is 400 ° C, and the time is 4 hours, and the alkali metal composite iron molybdenum sulfide catalyst MgxFey-Mo-S is finally obtained. According to different proportions, respectively recorded as Mg 3 Fe 1 Mo-S, Mg 2 Fe 1 Mo-S, Mg 1 Fe 1 Mo-S, Mg 1 Fe 2 Mo-S, Mg 1 Fe 3 Mo-S.

[0041] The XRD of the catalyst prepared under this condition is shown in figure 2 As shown, MoS was not observed in the end 2 diffra...

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Abstract

The invention provides a combined alkaline iron-molybdenum sulfide catalyst, a preparation method of the catalyst and an application of the catalyst to aromatic phenol and ether conversion. The catalyst is expressed by the aid of a molecular formula of MgxFey-Mo-S, x and y represent atomic ratio, and x: y = 3:1-1:3. MgxFey hydrotalcite serves as a precursor, the precursor is roasted at the temperature ranging from 350 DEG C to 500 DEG C to obtain oxide of MgxFey, the oxide and water solution with excessive MoO4<2>- ions are hydrated to obtain an MgxFey-MoO4<2> precursor of an intercalation layer, the MgxFey-MoO4<2> precursor is vulcanized through H2S / H2 mixed gas at the temperature ranging from 400 DEG C to 800 DEG C to finally obtain the MgxFey-Mo-S catalyst. The catalyst is effectively applied to aromatic phenol and ether conversion, cleavage of aryl-ether bands in a reactant is achieved, phenol products with low oxygen content are acquired, and the added value of the catalyst is improved.

Description

technical field [0001] The invention belongs to the technical field of industrial catalysis and bioenergy conversion, and relates to the preparation of metal sulfide catalysts, in particular to a method for preparing composite basic iron-molybdenum sulfide catalysts. Background technique [0002] With the deepening of human understanding of environmental pollution and resource crisis, the renewable and degradable properties of natural polymers have attracted increasing attention. Biomass, as a natural polymer, has many outstanding advantages compared to fossil energy, such as abundant reserves, carbon neutrality, easy access, zero emissions, and the only renewable resource that can be converted into liquid fuels. Among them, woody biomass is an important part of biomass energy, which is mainly composed of organic matter such as cellulose (40-50%), hemicellulose (25-35%) and lignin (15-20%). Due to the complex structure of lignin and its difficult to degrade, high-value util...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/051C07C37/00C07C39/06C07C37/11C07C37/50C07C39/04C07C1/22C07C15/02C07C13/20C07C41/01C07C43/215C07C41/20C07C43/23C07C37/055
CPCB01J27/0515C07C1/22C07C37/003C07C37/055C07C37/11C07C37/50C07C41/01C07C41/20C07C39/06C07C39/04C07C15/02C07C13/20C07C13/18C07C43/215C07C43/23C07C39/08C07C43/2055Y02P20/52
Inventor 纪娜刁新勇张晴黄艺博张罗云刘庆岭宋春风
Owner TIANJIN UNIV
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