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Atomic-scale monodispersed rhodium-based catalyst, preparation method thereof and application of atomic-scale monodispersed rhodium-based catalyst in preparation of methyl acetate through methanol gas-phase carbonylation

A monodisperse, atomic-level technology, applied in the fields of carbon monoxide or formate reaction preparation, chemical instruments and methods, physical/chemical process catalysts, etc. problems such as loss, to achieve the effect of high activity ratio homogeneous, reduced dosage and good stability

Active Publication Date: 2020-05-26
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

(2) Dimethyl ether is synthesized by carbonylation on the H-MOR molecular sieve catalyst, but the molecular sieve is prone to carbon deposition and deactivation, and the space-time yield is very low
(3) When methanol carbonylation prepares acetic acid, methyl acetate exists as a by-product, but the selectivity is low and the separation cost is high
However, the homogeneous catalyst system has shown certain shortcomings since its birth, such as the easy loss of noble metal catalysts, difficulty in separating the product from the catalyst, and complex catalyst recycling and recovery.

Method used

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  • Atomic-scale monodispersed rhodium-based catalyst, preparation method thereof and application of atomic-scale monodispersed rhodium-based catalyst in preparation of methyl acetate through methanol gas-phase carbonylation
  • Atomic-scale monodispersed rhodium-based catalyst, preparation method thereof and application of atomic-scale monodispersed rhodium-based catalyst in preparation of methyl acetate through methanol gas-phase carbonylation
  • Atomic-scale monodispersed rhodium-based catalyst, preparation method thereof and application of atomic-scale monodispersed rhodium-based catalyst in preparation of methyl acetate through methanol gas-phase carbonylation

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] The preparation of embodiment 1 catalyst sample

[0068] Rhodium source and additive element M source are dissolved in the deionized water of 15ml, obtain mixed solution, then 10.0g activated carbon (coconut shell charcoal, specific surface area is 1000m 2 / g, with an average particle size of 50um) immersed in the mixed solution. Evaporate the solvent in a water bath at 90°C, dry in an oven at 120°C for 8 hours, and roast at 300°C under nitrogen protection for 4 hours to obtain the precursor. The precursor is placed in a mixed atmosphere of carbon monoxide and halogenated alkanes for post-treatment to obtain the atomic-level monodisperse rhodium-based catalyst.

[0069] The relationship between the sample numbers of the obtained samples and the preparation conditions is shown in Table 1.

[0070] Table 1

[0071]

[0072]

[0073] *: Calculated by mass percentage of rhodium element in the catalyst.

Embodiment 2

[0074] The characterization of embodiment 2 catalyst sample

[0075] The samples obtained in Example 1 were characterized by transmission electron microscopy and spherical aberration electron microscopy, and the results showed that in the samples prepared in Example 1, rhodium was dispersed in the rhodium-based catalyst in the form of mononuclear complexes .

[0076] Among them, the sample Rh 1 -La / AC-1 is a typical representative, and its ordinary electron microscope photos are as follows figure 1 As shown, its spherical aberration electron microscope photo is shown as figure 2 shown. From figure 1 It can be found that: under the macroscopic scale with the highest resolution of 50nm in the ordinary electron microscope, the supported nano-metal particles cannot be seen in the carrier activated carbon; in the further spherical aberration electron microscope photos, the metal catalyst dispersed at the single atomic level can be clearly seen.

[0077] The test results of th...

Embodiment 3

[0078] Embodiment 3 methanol vapor phase carbonylation prepares methyl acetate reaction

[0079] The catalyst (0.3 g) obtained in Example 1, with an average particle size of 500 μm, was placed in a fixed-bed quartz tube reactor, and 20-40 mesh quartz sand was loaded at both ends. Then the temperature was raised from room temperature to 240°C at a rate of 5°C / min, and H 2 , CO, methanol, and methyl iodide (molar ratio CO / H 2 =10, molar ratio CO / CH 3 OH=1, mass ratio CH 3 OH / CH 3 I=7 / 3), reaction pressure 1.7MPa, methanol liquid hourly volume space velocity 12h -1 The reaction was stable for 24 hours under certain conditions, and the conversion rate of methanol and the selectivity of methyl acetate were analyzed and calculated online. The results are shown in Table 2.

[0080] Table 2

[0081] catalyst Methanol conversion (%) Methyl acetate selectivity*(%) Rh 1 -La / AC-1

[0082] *Based on methanol converted, other products are mainly acetic acid.

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Abstract

The invention discloses an atomic-scale monodispersed rhodium-based catalyst which is characterized by comprising an active component, an auxiliary component and a carrier activated carbon, wherein the active component comprises a rhodium element, and the active component comprises an auxiliary agent element M; and the rhodium element is monodispersed on the carrier activated carbon in the form ofa mononuclear complex. The catalyst has the advantages of higher activity than a homogeneous catalyst, single-point active site, no need of transition period in reaction, good catalyst stability andthe like. The catalyst is used for preparing methyl acetate through gas-phase carbonylation of methanol, and can be used for preparing methyl acetate with high activity and high selectivity.

Description

technical field [0001] The application relates to an atomic-level monodisperse rhodium-based catalyst, its preparation method and its application in the gas-phase carbonylation of methanol to prepare methyl acetate, which belongs to the field of industrial catalysis. Background technique [0002] Methyl acetate will gradually replace acetone, butanone, ethyl acetate, cyclopentane, etc. Because it does not belong to the emission of organic pollutants that are restricted in use, it can meet the new environmental protection standards for paint, ink, resin, and adhesive factories. The hydrogenation of methyl acetate to ethanol is also one of the main ways to produce ethanol from coal. Its preparation methods mainly include (1) acetic acid and methanol are directly esterified with sulfuric acid as a catalyst to form a crude methyl acetate product, and then dehydrated with calcium chloride, neutralized with sodium carbonate, and fractionated to obtain a finished product of methyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/63B01J23/648B01J23/60B01J23/89B01J23/656B01J23/46B01J23/58C07C67/36C07C69/14
CPCB01J23/464B01J23/58B01J23/60B01J23/63B01J23/6484B01J23/6562B01J23/8906C07C67/36C07C69/14
Inventor 丁云杰冯四全宋宪根
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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